Compound, composition, encapsulation film and semiconductor device for encapsulation film
By using a composition containing silicon monomer, photocuring monomer and photocrosslinking initiator, a high-light transmissibility and low-permeability packaging film is formed, which solves the problem of water vapor and oxygen permeation in OLED device packaging and extends the use of the device Lifespan and improves its reliability.
Patent Information
- Application Number
- CN202210652641.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-10
- Publication Date
- 2024-12-13
- Estimated Expiration
- 2042-06-10
AI Technical Summary
It is urgent to effectively prevent the penetration of water vapor and oxygen from being impervious to the packaging technology of existing OLED devices while ensuring light transmission and long service life.
Using a composition containing silicon monomer, photocuring monomer and photocrosslinking initiator, the encapsulated film is formed by photocuring. The composition has high light transmittance, long life and low plasma etching rate, which can be effectively Barrier water vapor and oxygen and extend the service life of OLED devices.
Achieve higher light transmittance, faster curing speed and lower water vapor and oxygen transmittance, improving the reliability and service life of OLED devices while avoiding shrinkage volume of organic ink compositions when curing Increase.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of thin film packaging, and in particular relates to a compound, a composition, a packaging film and a semiconductor device for packaging thin films. Background Art
[0002] OLED (Organic Light Emitting Diode), also known as organic laser display, organic light-emitting semiconductor (Organic Electroluminescent Display, OLED). It is a current-type organic light-emitting device, which is a phenomenon of luminescence caused by the injection and recombination of carriers. The luminescence intensity is proportional to the injected current. Under the action of the electric field, the holes generated by the anode and the electrons generated by the cathode will move, inject into the hole transport layer and the electron transport layer respectively, and migrate to the light-emitting layer. When the two meet in the light-emitting layer, energy excitons are generated, thereby exciting the light-emitting molecules to finally produce visible light. The organic light-emitting display device includes an organic light-emitting device (OLED) composed of a hole injection electrode (anode), an organic light-emitting layer, and an electron injection electrode (cathode). This organic light-emitting device is usually provided on a glass substrate, and in order to prevent deterioration caused by the influx of moisture or oxygen from the outside, it is covered with another substrate. Recently, display devices including organic light-emitting display devices have become thinner and thinner under the demand of consumers. In order to meet this demand, thin film encapsulation (Thin Film Encapsulation; TFE) is applied to the covering of organic light-emitting devices.
[0003] For OLED devices, if their service life is to reach more than 10,000 hours, the water vapor transmission rate (WVTR) of the device must be less than 10 -6 g / m 2 / day, oxygen permeability (OTR) less than 10 -5 g / (m 2 ·d), which is a great challenge to the sealing structure of display devices, so it is necessary to develop suitable OLED packaging technology.
[0004] The purpose of OLED packaging is to isolate the light-emitting device from the environment to prevent the intrusion of harmful substances such as moisture and oxygen, and to prevent damage from external forces, stabilize various parameters of the device, and thus increase the service life of the OLED. OLED packaging mainly includes cover packaging, filler packaging, laser packaging, thin film packaging and other methods.
[0005] Traditional cover packaging is to use epoxy resin to bond the prepared substrate and cover together in a glove box filled with inert gas to form a closed space to isolate the device from the external environment. Water, oxygen and other components in the air can only penetrate into the device through the epoxy resin, which effectively prevents the contact of water and oxygen in the air with the functional layers of the OLED. The material of the packaging cover is generally glass or metal, but the opacity of the metal cover limits its application in device packaging. Although glass cover packaging does not have the problem of light transmittance, it has poor toughness and is fragile, so solving this problem is urgent. Summary of the invention
[0006] The object of the present invention is to provide a compound, a composition, a packaging film and a semiconductor device for packaging films. The packaging film prepared by the compound of the present invention has good light transmittance and long service life.
[0007] The present invention provides a compound for encapsulating a thin film, having a structure shown in Formula I:
[0008] Formula 1;
[0009] wherein X1 is selected from hydrogen, substituted or unsubstituted C1 to C10 alkyl, substituted or unsubstituted C3 to C20 cycloalkyl, substituted or unsubstituted C1 to C10 hydroxyalkyl, substituted or unsubstituted C6 to C20 aryl, substituted or unsubstituted 2-20 membered heteroaryl, substituted or unsubstituted C2 to C10 alkenyl, substituted or unsubstituted C1 to C10 alkoxy, substituted or unsubstituted lactone, substituted or unsubstituted carboxyl, substituted or unsubstituted glycidyl ether or hydroxyl;
[0010] R1 and R2 are alkyl groups with the same or different carbon atoms;
[0011] R3, R4, R5 and R6 are each independently selected from hydrogen, C1-C20 alkyl, C1-C20 alkoxy, C1-C10 alkenyl, C1-C10 alkynyl, C6-C30 arylene, C3-C20 cycloalkyl or 4-30 membered heteroaryl;
[0012] A is selected from O, S, NR, substituted or unsubstituted C1~C10 alkyl, substituted or unsubstituted C6~C20 aryl, wherein R in NR is hydrogen, substituted or unsubstituted C1~C20 alkyl, substituted or unsubstituted C1~C20 alkoxy, C6~C30 aryl or 4~30 membered heteroaryl;
[0013] Y1 is any one selected from Formula 2 to Formula 4,
[0014]
[0015] X2 is a substituted acrylate group or an unsubstituted acrylate group, and the general structural formula is Formula 5,
[0016] ;
[0017] Wherein, * is the connection position, and Z is selected from H, a substituted or unsubstituted alkyl group having less than 20 carbon atoms, or an alkoxy group having less than 20 carbon atoms.
[0018] Preferably, X1 is selected from hydrogen, substituted or unsubstituted C1 to C5 alkyl, substituted or unsubstituted C3 to C15 cycloalkyl, substituted or unsubstituted C1 to C5 hydroxyalkyl, substituted or unsubstituted C6 to C12 aryl, substituted or unsubstituted 2-12 membered heteroaryl, substituted or unsubstituted C2 to C5 alkenyl, substituted or unsubstituted C1 to C5 alkoxy, substituted or unsubstituted lactone, substituted or unsubstituted carboxyl, substituted or unsubstituted glycidyl ether or hydroxyl;
[0019] R1 and R2 are each independently selected from a C1-C5 alkyl group;
[0020] R3, R4, R5 and R6 are each independently selected from hydrogen, C1-C10 alkyl, C1-C10 alkoxy, C1-C6 alkenyl, C1-C6 alkynyl, C6-C20 arylene, C3-C10 cycloalkyl or 4-20 membered heteroaryl;
[0021] A is selected from O, S, NR, substituted or unsubstituted C1~C5 alkyl, substituted or unsubstituted C6~C10 aryl, wherein R in NR is hydrogen, substituted or unsubstituted C1~C10 alkyl, substituted or unsubstituted C1~C10 alkoxy, C6~C20 aryl or 4~20 membered heteroaryl;
[0022] Z is selected from H, a substituted or unsubstituted alkyl group having less than 10 carbon atoms, or an alkoxy group having less than 10 carbon atoms.
[0023] Preferably, the X1 is selected from methyl or phenethyl;
[0024] R1 and R2 are each independently selected from ethyl or propyl;
[0025] Said R3, R4, R5 and R6 are each independently selected from methyl or phenyl;
[0026] A is selected from O;
[0027] Z is selected from methyl.
[0028] Preferably, the compound is selected from any one of A01 to A09:
[0029] .
[0030] The present invention provides a composition for encapsulating a thin film, comprising the following components in weight fractions:
[0031] 15-80wt% of silicon-containing monomer, 1-10wt% of photocrosslinking initiator and 15-75wt% of photocurable monomer;
[0032] The silicon-containing monomer is the compound used for encapsulation thin film as described above.
[0033] Preferably, the photocrosslinking initiator is selected from one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenylacetone and 2,4,6-trimethylbenzoyl diphenylphosphite;
[0034] The photocurable monomer includes one or more of monofunctional (meth)acrylate of C1 to C30 monohydric alcohol or polyhydric alcohol, difunctional (meth)acrylate of C2 to C30 monohydric alcohol or polyhydric alcohol, and multifunctional (meth)acrylate of C3 to C30 monohydric alcohol or polyhydric alcohol.
[0035] Preferably, the monofunctional (meth)acrylate of the C1 to C30 monohydric alcohol or polyhydric alcohol includes one or more of lauryl acrylate, ethoxyethoxyethyl acrylate, butyl acrylate, hydroxyethyl acrylate, isobornyl acrylate, ethoxylated tetrahydrofuran acrylate, methacrylate phosphate and isobornyl methacrylate;
[0036] The difunctional (meth)acrylate of C2 to C30 monohydric alcohol or polyhydric alcohol includes one or more of diethylene glycol diacrylate, triethylene glycol diacrylate, ethylene glycol diacrylate, polyethylene glycol (200) diacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (600) diacrylate, neopentyl glycol diacrylate, propoxy neopentyl glycol diacrylate, 1,6-hexanediol diacrylate, 1,4-butanediol diacrylate, 20 (ethoxy) bisphenol A diacrylate and glycerol diacrylate;
[0037] The multifunctional (meth)acrylate of C3 to C30 monohydric alcohol or polyhydric alcohol includes one or more of trimethylolpropane triacrylate, pentaerythritol triacrylate, trihydroxymethylpropane triol triacrylate, trimethylolpropane triacrylate, propoxylated trimethylolpropane triacrylate, pentaerythritol tripropylene and propoxylated pentaerythritol propylene, di(trimethylolpropane) tetraacrylate, triethylene glycol dimethacrylate, long-chain aliphatic hydrocarbon glycidyl ether acrylate, dipentaerythritol hexaacrylate, tripropylene glycol diacrylate, diethyl phthalate diacrylate, ethoxylated trimethylolpropane triol triacrylate, propoxylated trimethylolpropane triol triacrylate, propoxylated glycerol triacrylate, tri(2-hydroxyethyl)isocyanuric acid triacrylate and ethoxylated neopentyl glycol methoxy monoacrylate.
[0038] The present invention provides a packaging film, which is formed by photocuring the composition for packaging film mentioned above.
[0039] The present invention provides a semiconductor device, comprising the packaging film mentioned above.
[0040] Preferably, the semiconductor device is an electroluminescent device, a photoluminescent device, a lighting device, a light emitting diode, a solar cell, a thin film transistor or a photodetector.
[0041] The present invention provides a compound for encapsulating thin films, which uses a curable silicon-containing monomer having the above-mentioned general formula 1 as a polymerized monomer. Due to the benzene ring and epoxy group contained therein, when it is combined with a curable epoxyalkyl diluent, the formed polymer film has higher light transmittance, higher curing speed, and lower plasma etching rate, thereby better meeting the requirements of encapsulating thin films in the prior art.
[0042] The composition for encapsulating thin film in the present invention is composed of silicon-containing monomers, photocurable monomers and photoinitiators. Since the silicon-containing monomers contain rigid group Si atoms in their molecular structure, they have better heat resistance, transparency, lower water vapor permeability and oxygen permeability than ink compositions without silicon atoms. On the other hand, they also reduce the excessive shrinkage volume generated by the organic ink composition during curing. When used for thin film encapsulation of OLED devices, they can effectively block water and oxygen, improve reliability, and further extend the service life of OLED devices. DETAILED DESCRIPTION
[0043] The present invention provides a compound for encapsulating a thin film, having a structure shown in Formula I:
[0044] Formula 1;
[0045] wherein X1 is selected from hydrogen, substituted or unsubstituted C1 to C10 alkyl, substituted or unsubstituted C3 to C20 cycloalkyl, substituted or unsubstituted C1 to C10 hydroxyalkyl, substituted or unsubstituted C6 to C20 aryl, substituted or unsubstituted 2-20 membered heteroaryl, substituted or unsubstituted C2 to C10 alkenyl, substituted or unsubstituted C1 to C10 alkoxy, substituted or unsubstituted lactone, substituted or unsubstituted carboxyl, substituted or unsubstituted glycidyl ether or hydroxyl;
[0046] Preferably, X1 is selected from hydrogen, substituted or unsubstituted C1, C2, C3, C4 or C5 alkyl, substituted or unsubstituted C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14 or C15 cycloalkyl, substituted or unsubstituted C1, C2, C3, C4 or C5 hydroxyalkyl, substituted or unsubstituted C6, C7, C8, C9, C10, C11, C12, C13, C14 or C15 a substituted or unsubstituted 2-, 3-, 4-, 5-, 6-, 7-, 8-, 9-, 10-, 11- or 12-membered heteroaryl group, a substituted or unsubstituted C2, C3, C4 or C5 alkenyl group, a substituted or unsubstituted C1, C2, C3, C4 or C5 alkoxy group, a substituted or unsubstituted lactone group, a substituted or unsubstituted carboxyl group, a substituted or unsubstituted glycidyl ether group or a hydroxyl group;
[0047] More preferably, X1 is selected from methyl or phenethyl.
[0048] R1 and R2 are alkyl groups having the same or different carbon atoms. Preferably, R1 and R2 are each independently selected from C1, C2, C3, C4 or C5 alkyl groups. More preferably, R1 and R2 are each independently selected from ethyl or propyl groups.
[0049] R3, R4, R5 and R6 are each independently selected from hydrogen, C1-C20 alkyl, C1-C20 alkoxy, C1-C10 alkenyl, C1-C10 alkynyl, C6-C30 arylene, C3-C20 cycloalkyl or 4-30 membered heteroaryl;
[0050] Preferably, R3, R4, R5 and R6 are each independently selected from hydrogen, C1, C2, C3, C4, C5, C6, C7, C8, C9 or C10 alkyl, C1, C2, C3, C4, C5, C6, C7, C8, C9 or C10 alkoxy, C1, C2, C3, C4, C5 or C6 alkenyl, C1, C2, C3, C4, C5 or C6 alkynyl, C1, C2, C3, C4, C5 or C6 alkynyl, C7, C8, C9 or C10 alkyl, C1, C2, C3, C4, C5 or C6 alkenyl, C1, C2, C3, C4, C5 or C6 alkynyl, 9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, or C20 arylene, C3, C4, C5, C6, C7, C8, C9, or C10 cycloalkyl, or a 4-, 5-, 6-, 7-, 8-, 9-, 10-, 11-, 12-, 13-, 14-, 15-, 16-, 17-, 18-, 19-, or 20-membered heteroaryl;
[0051] More preferably, R3, R4, R5 and R6 are each independently selected from methyl or phenyl.
[0052] A is selected from O, S, NR, substituted or unsubstituted C1~C10 alkyl, substituted or unsubstituted C6~C20 aryl, wherein R in NR is hydrogen, substituted or unsubstituted C1~C20 alkyl, substituted or unsubstituted C1~C20 alkoxy, C6~C30 aryl or 4~30 membered heteroaryl;
[0053] Preferably, A is selected from O, S, NR, substituted or unsubstituted C1, C2, C3, C4 or C5 alkyl, substituted or unsubstituted C6, C7, C8, C9 or C10 aryl, wherein R in NR is hydrogen, substituted or unsubstituted C1, C2, C3, C4, C5, C6, C7, C8, C9 or C10 alkyl, substituted or unsubstituted C1, C2, C3, C4, C5, C6, C7, C8, C9 or C10 aryl, 7, C8, C9, or C10 alkoxy, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, or C20 aryl, or a 4-, 5-, 6-, 7-, 8-, 9-, 10-, 11-, 12-, 13-, 14-, 15-, 16-, 17-, 18-, 19-, or 20-membered heteroaryl;
[0054] More preferably, A is selected from O.
[0055] Y1 is any one selected from Formula 2 to Formula 4,
[0056] ;
[0057] X2 is a substituted acrylate group or an unsubstituted acrylate group, and the general structural formula is Formula 5,
[0058] ;
[0059] Wherein, * is the connection position, and Z is selected from H, a substituted or unsubstituted alkyl group having less than 20 carbon atoms, or an alkoxy group having less than 20 carbon atoms; preferably, Z is selected from a methyl group.
[0060] Preferably, the above compound is selected from any one of A01 to A09:
[0061] .
[0062] The compound represented by Formula 1 in the present invention is used for thin film encapsulation. Based on this, the present invention also provides a composition for preparing an encapsulation film, comprising 15-80 wt % of a silicon-containing monomer, 1-10 wt % of a photocrosslinking initiator and 15-75 wt % of a photocurable monomer;
[0063] The silicon-containing monomer is the compound used for encapsulation thin film mentioned above, and the present invention will not be described in detail here.
[0064] In the present invention, the mass fraction of the silicon-containing monomer is preferably 15-80wt%, more preferably 20-75wt%, such as 15wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt%, 45wt%, 50wt%, 55wt%, 60wt%, 65wt%, 70wt%, 75wt%, 80wt%, preferably a range value with any of the above values as the upper or lower limit.
[0065] In the present invention, the photocrosslinking initiator is preferably one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenylacetone and 2,4,6-trimethylbenzoyl diphenyl phosphite; the mass fraction of the photocrosslinking initiator is preferably 1-10wt%, more preferably 3-8wt%, such as 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, preferably a range value with any of the above values as the upper or lower limit.
[0066] In the present invention, the photocurable monomer is preferably one or more of a monofunctional (meth)acrylate of a C1 to C30 monohydric alcohol or polyhydric alcohol, a difunctional (meth)acrylate of a C2 to C30 monohydric alcohol or polyhydric alcohol, and a multifunctional (meth)acrylate of a C3 to C30 monohydric alcohol or polyhydric alcohol;
[0067] The monofunctional (meth)acrylate of the C1 to C30 monohydric alcohol or polyhydric alcohol includes one or more of lauryl acrylate (LA), ethoxyethoxyethyl acrylate (EOEOEA)- KPX A007, butyl acrylate (BA), hydroxyethyl acrylate, isobornyl acrylate, ethoxylated tetrahydrofuran acrylate (THF(EO)A)- KPX A015, methacrylate phosphate and isobornyl methacrylate;
[0068] The difunctional (meth)acrylate of the C2 to C30 monohydric alcohol or polyhydric alcohol includes a difunctional (meth)acrylate of a dihydric alcohol structure, such as one or more of ethylene glycol diacrylates and propylene glycol diacrylates, specifically one or more of diethylene glycol diacrylate (DEGDA), triethylene glycol diacrylate (TEGDA), ethylene glycol diacrylate, polyethylene glycol (200) diacrylate [PEG (200) DA], polyethylene glycol (400) diacrylate [PEG (400) DA], polyethylene glycol (600) diacrylate [PEG (600) DA], neopentyl glycol diacrylate and propoxy neopentyl glycol diacrylate, 1,6-hexanediol diacrylate (HDDA), 1,4-butanediol diacrylate (BDDA), 20 (ethoxy) bisphenol A diacrylate [BPA (EO) 20DA] and propylene glycol diacrylate (TPGDA).
[0069] The multifunctional (meth)acrylate of the C3 to C30 monohydric alcohol or polyhydric alcohol includes trimethylolpropane triacrylate (TMPTA), pentaerythritol triacrylate (PETA), trimethylolpropane triol triacrylate (TMPTMA), trimethylolpropane triacrylate, propoxylated trimethylolpropane triacrylate, pentaerythritol tripropylene glycol ester and propoxylated pentaerythritol propenyl glycol ester, di(trimethylolpropane) tetraacrylate, triethylene glycol dimethacrylate, long-chain aliphatic hydrocarbon glycidyl ether acrylate, One or more of dipentaerythritol hexaacrylate, tripropylene glycol diacrylate, diethyl phthalate diacrylate (PDDA), ethoxylated trihydroxymethylpropane triol triacrylate [TMP(EO)TMA], propoxylated trihydroxymethylpropane triol triacrylate [TMP(PO)TMA], propoxylated glycerol triacrylate [G(PO)TA], tris(2-hydroxyethyl)isocyanuric acid triacrylate and ethoxylated neopentyl glycol methoxy monoacrylate [TMP(PO)MEDA].
[0070] In the present invention, the mass fraction of the photocurable monomer is preferably 15~75wt%, more preferably 20~70wt%, such as 15wt%, 20 wt%, 25 wt%, 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, 75 wt%, preferably a range value with any of the above values as the upper or lower limit.
[0071] The present invention also provides an encapsulation film for encapsulating an OLED device, wherein the composition for preparing the encapsulation film described above is subjected to UV (100 mW / cm 2 10s) photocuring.
[0072] The present invention also provides a semiconductor device, comprising a functional structure and the packaging film described above, wherein the semiconductor device is an electroluminescent device, a photoluminescent device, a lighting device, a light emitting diode, a solar cell, a thin film transistor or a photodetector.
[0073] The present invention provides a compound for encapsulating thin films, which uses a curable silicon-containing monomer having the above-mentioned general formula 1 as a polymerized monomer. Due to the benzene ring and epoxy group contained therein, when it is combined with a curable epoxyalkyl diluent, the formed polymer film has higher light transmittance, higher curing speed, and lower plasma etching rate, thereby better meeting the requirements of encapsulating thin films in the prior art.
[0074] The composition for encapsulating thin film in the present invention is composed of silicon-containing monomers, photocurable monomers and photoinitiators. Since the silicon-containing monomers contain rigid group Si atoms in their molecular structure, they have better heat resistance, transparency, lower water vapor permeability and oxygen permeability than ink compositions without silicon atoms. On the other hand, they also reduce the excessive shrinkage volume generated by the organic ink composition during curing. When used for thin film encapsulation of OLED devices, they can effectively block water and oxygen, improve reliability, and further extend the service life of OLED devices.
[0075] In order to further illustrate the present invention, a compound for encapsulation film, a composition, an encapsulation film and a semiconductor device provided by the present invention are described in detail below in combination with embodiments, but it should not be understood as limiting the scope of protection of the present invention.
[0076] Embodiment 1: A method for preparing an encapsulation film, comprising the following steps:
[0077] Preparation of silicon-containing monomer A01:
[0078] Dissolve 1000g of pentamethyldisiloxane A and 900g of allyl alcohol B in 10L of ethyl acetate, add to the reactor, add 6g of the Custer catalyst solution of tetramethyldivinyldisiloxane to the reaction system, heat to 80°C, reflux and stir for 6 hours. After the temperature is lowered to room temperature, filter to remove the Pt catalyst, use a vacuum distillation device to remove the solvent and residual allyl alcohol, and obtain 800g of chemical formula C. Add 800g of compound C to 6L of toluene, add 1720g of ethyl isocyanate acrylate, and stir at 50°C for 4 hours. Silicon-containing monomer A01 is obtained.
[0079] Mass spectrum: calculated value is 361.59; measured value is 361.56
[0080] Elemental analysis: Calculated values: C, 49.83; H, 8.64; N, 3.87; O, 22.12; Si, 15.53; Found values: C, 49.81; H, 8.66; N, 3.83; O, 22.14; Si, 15.55
[0081]
[0082] Step S1: Processing of organic layer materials
[0083] The silicon-containing monomer A01, the photocurable monomer diethylene glycol diacrylate, and the crosslinking initiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide;
[0084]
[0085] Weigh 20 g of A01, 75 g of diethylene glycol diacrylate and 5 g of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, mix them together, stir them under vacuum at 50° C. for 80 h, filter them with a syringe filter, and detect them with a particle counter. When no more than 50 particles with a particle size greater than 0.5 μm are detected, a treated organic layer material is obtained;
[0086] Step S2: Selecting silicon nitride as the inorganic layer material;
[0087] Step S3: Preparation of inorganic layer
[0088] Applying an inorganic layer material on the surface of the object to be encapsulated by a CVD method to form an inorganic layer;
[0089] Step S4: Preparation of organic layer
[0090] The treated organic layer material was sprayed on the surface of the inorganic layer with an inkjet printer to form an organic layer. 2, 10 seconds of ultraviolet light exposure each time promotes the hardening of the organic layer;
[0091] Step S5: Formation of encapsulation film
[0092] The surface of the object to be encapsulated is deposited and coated in the form of alternating inorganic layers, organic layers, and inorganic layers. Finally, the inorganic layers and organic layers, and the inorganic layers, deposited and coated on the surface of the object to be encapsulated are the encapsulation film. Example 2
[0093] In step S1: the silicon-containing monomer A01 is replaced by A02, the photocurable monomer diethylene glycol diacrylate is replaced by 1,6-hexanediol diacrylate, and the crosslinking initiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide is replaced by 2-hydroxy-2-methyl-1-phenylacetone, and the rest is the same as in Example 1. Example 3
[0094] In step S1: the silicon-containing monomer A01 is replaced by A03, the photocurable monomer diethylene glycol diacrylate is replaced by diethylene phthalate diacrylate, and the crosslinking initiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide is replaced by 2-hydroxy-2-methyl-1-phenylacetone. Others are the same as in Example 1.
[0095] Embodiment 4: A method for preparing an encapsulation film,
[0096] In step S1: the silicon-containing monomer A01 is replaced by A04, the photocurable monomer diethylene glycol diacrylate is replaced by propoxylated glycerol triacrylate, and the crosslinking initiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide is replaced by 2,4,6-trimethylbenzoyl diphenylphosphinate, and the rest is the same as in Example 1. Example 4
[0097] In step S1 , 20 g of silicon-containing monomer A01 is replaced by 30 g of silicon-containing monomer A01, and 75 g of diethylene glycol diacrylate is replaced by 60 g of diethylene glycol diacrylate. Other steps are the same as those in Example 1. Example 5
[0098] In step S1: 20 g of silicon-containing monomer A02 is replaced by 30 g of silicon-containing monomer A02, 75 g of 1,6-hexanediol diacrylate is replaced by 60 g of 1,6-hexanediol diacrylate, and the rest is the same as in Example 2. Example 6
[0099] In step S1 , 20 g of silicon-containing monomer A03 is replaced by 30 g of silicon-containing monomer A03 , 75 g of diethyl phthalate diacrylate is replaced by 60 g of diethyl phthalate diacrylate , and the rest is the same as in Example 3. Example 7
[0100] In step S1: 20 g of silicon-containing monomer A04 is replaced by 30 g of silicon-containing monomer A04, 75 g of propoxylated glycerol triacrylate is replaced by 60 g of propoxylated glycerol triacrylate, and the rest is the same as in Example 4.
[0101] Comparative Example 1
[0102] The mass of the silicon-containing monomer A01 in the above embodiment 1 is 0 g, the mass fraction of the photocurable monomer diethylene glycol diacrylate is changed to 98 g, and the mass fraction of the initiator 2,4,6-trimethylbenzoyl-diphenylphosphine oxide is changed to 2 g, the mixture is mixed together, stirred for 80 hours under vacuum at 50°C, and then filtered with a syringe filter. The mixture is measured using a particle counter, and when the number of particles with a particle size greater than 0.5 μm is detected to be no more than 50, a photocurable composition is obtained.
[0103] Test Example 1
[0104] The encapsulation films of Examples 1-8 and Comparative Example 1 were tested for water vapor transmission rate. The testing instrument was a high-precision water vapor transmission rate tester of AQUARAN2 manufactured by MOCON Corporation (USA). The testing conditions were: temperature 85° C., relative humidity 85%; and testing time: 24 hours.
[0105] The light transmittance of the encapsulation films of Examples 1 to 8 and Comparative Example 1 was tested using a light transmittance tester under the following conditions: a temperature of 40° C. and a relative humidity of 85%. The results are shown in Table 1.
[0106]
[0107] The water vapor permeability of the encapsulation films prepared in Examples 1-8 and Comparative Example 1 was tested, wherein the water vapor permeability of the encapsulation films after adding the composition monomer was significantly lower than that of the encapsulation films without adding the composition monomer. The above problem can also be explained by comparing the embodiments in Table 1. The organic light-emitting device encapsulated by the above encapsulation film can effectively isolate water vapor and extend the practical life of the organic light-emitting device.
[0108] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A compound for encapsulating thin films, having a structure shown in Formula A01:
2. A composition for encapsulation film, comprising the following components in mass fractions: 15-80 wt% of silicon-containing monomer, 1-10 wt% of photocrosslinking initiator and 15-75 wt% of photocurable monomer; The silicon-containing monomer is the compound for encapsulating thin films as claimed in claim 1.
3. The composition according to claim 2, characterized in that The photocrosslinking initiator is selected from one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenylacetone and 2,4,6-trimethylbenzoyl diphenylphosphite; The photocurable monomer includes one or more of monofunctional (meth)acrylate of C1 to C30 monohydric alcohol or polyhydric alcohol, difunctional (meth)acrylate of C2 to C30 monohydric alcohol or polyhydric alcohol, and multifunctional (meth)acrylate of C3 to C30 monohydric alcohol or polyhydric alcohol.
4. The composition according to claim 3, characterized in that The monofunctional (meth)acrylate of the C1 to C30 monohydric alcohol or polyhydric alcohol includes one or more of lauryl acrylate, ethoxyethoxyethyl acrylate, butyl acrylate, hydroxyethyl acrylate, isobornyl acrylate, ethoxylated tetrahydrofuran acrylate, methacrylate phosphate and isobornyl methacrylate; The difunctional (meth)acrylate of C2 to C30 monohydric alcohol or polyhydric alcohol includes one or more of diethylene glycol diacrylate, triethylene glycol diacrylate, ethylene glycol diacrylate, polyethylene glycol (200) diacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (600) diacrylate, neopentyl glycol diacrylate, propoxy neopentyl glycol diacrylate, 1,6-hexanediol diacrylate, 1,4-butanediol diacrylate, 20 (ethoxy) bisphenol A diacrylate and glycerol diacrylate; The multifunctional (meth)acrylate of C3 to C30 monohydric alcohol or polyhydric alcohol includes one or more of trimethylolpropane triacrylate, pentaerythritol triacrylate, trihydroxymethylpropane triol triacrylate, trimethylolpropane triacrylate, propoxylated trimethylolpropane triacrylate, pentaerythritol tripropylene and propoxylated pentaerythritol propylene, di(trimethylolpropane) tetraacrylate, triethylene glycol dimethacrylate, long-chain aliphatic hydrocarbon glycidyl ether acrylate, dipentaerythritol hexaacrylate, tripropylene glycol diacrylate, diethyl phthalate diacrylate, ethoxylated trimethylolpropane triol triacrylate, propoxylated trimethylolpropane triol triacrylate, propoxylated glycerol triacrylate, tri(2-hydroxyethyl)isocyanuric acid triacrylate and ethoxylated neopentyl glycol methoxy monoacrylate.
5. A packaging film formed by photocuring the composition for packaging film according to claim 2. 6 . A semiconductor device comprising the encapsulation film according to claim 5 .
7. The semiconductor device according to claim 6, characterized in that The semiconductor device is an electroluminescent device, a photoluminescent device, a lighting device, a light emitting diode, a solar cell, a thin film transistor or a photodetector.
